Dye composition and dyeing method



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The present invention relates to dyes. More in particular, the present invention relates to a dyeing method and a composition of dye liquor for dyeing yarn and cloth with highly dispersed vat dye pigments.

It is known in the art that great difficulties arise When trying to evenly and uniformly dye yarn and cloth so as to obtain a product with an entirely evenly colored appearance of all portions of the yarn or cloth. Hi herto it has not been possible to obtain such an evenly colored product with the known dye compositions and according to the known dyeing methods. W ere yarn i d ed on e yarn producing apparatus proper it has proved impossible to introduce the non-substantive dye pigment entirely into the yarn fibers during the padding operation. This leads to an unequal distribution of the dye pigment throughout the yarn fibers during the pigment reduction process. Where stretches of cloth are dyed an unequal distribution of the dye pigment throughout the fabric of the cloth is caused by the migration of the pigment during the intermediate drying process of the cloth. As the cloth frequently has portions of uneven density of the fiber structure the pigment migrates from the denser portions which dry comparatively slow to the thinner portions of the cloth drying much faster. Consequently, the finished product is very unevenly dyed in its various portions.

With the foregoing in mind, it is the general object of the present invention to provide for a dyeing method and a dye liquor containing highly dispersed vat dye pigments for dyeing yarn-s and pieces of cloth with which an entirely even and uniform distribution of the dye pigments throughout the yarn or cloth fibers is obtained and an even coloring effect is accomplished.

'It is a particular object of the present invention to provide for a dyeing method and a dye liquor containing highly dispersed vat dye pigments for dyeing yarns wherein the pigment of the dye liquor bath is entirely and fully utilized and evenly and uniformly distributed throughout the fiber structure of the yarn.

It is another particular object of the present invention to provide for a dyeing method and a dye liquor containing highly dispersed vat dye pigments for dyeing pieces of cloth whereby a migration and an unequal distribution of the pigment throughout the fiber structure of the cloth is safely prevented.

These objects are achieved by the present invention according to which the dyeing of yarn or pieces of cloth with highly dispersed vat dye pigment is effected in the presence of anionic, surfaceactive substances containing a hydrocarbon chain with at least 6 carbon atoms, and in the presence of acids, particularly organic acids. The hydrocarbon chain may also form a ring, but not more than one.

The dye liquor of the invention contains, in addition to the highly dispersed dye pigments and other substances known per se, anionic, surface-active substances with a hydrocarbon chain of at least 6 carbon atoms which may also form not more than one ring, as for example: Salts of alkyl sulfo acids, which can be obtained, in a manner known per se, by causing a reaction of aliphatic hydrocarbons with chlorine and sulfur dioxide, thereby obtaining a suite chloride, and, saponifying the latter.

3,978,13fi Patented Feb. 19, 1963 As a surface-active substance of the group indicated it is also possible to use, for example, salts of the sulfuric acid esters of oxystearic acid amides, or salts of sulfo succinic acid esters, salts of alkylated benzene sulfo acids. Instead of the salts of sulfonates it is also possible to use the corresponding sulfo acids.

The dye liquor further contains acids, particularly organic acids as, for example, formic acid, acetic acid, glycolic acid, lactic acid, halogenated carbonic acids, aromatic sulfonic acids, preferably benzene and toluene sulfonic acids. It has been found that non-volatile organic acids are particularly useful. The pH of the dye liquor is between 2 and 4, preferably between 2.5 and 3.

According to the dyeing method of the present invention, yarn is dyed by preparing a dye liquor of a composition known per se, and adding thereto the aforedescribed substances, subjecting the yarn to the dyeing liquor until substantially all pigment has been removed from the liquor. In the case of dyeing pieces of cloth, a dye pigment suspension of a composition known per se is prepared to which there are added the aforedescribed substances, whereupon the cloth is padded with this pigment suspension, and then subjected to an intermediate drying process, which does not cause any migration of the pigment.

The invention is further described with reference to the following examples which are, of course, not to be considered as limitative of the scope or applicability of the present invention.

Example I 300 kilograms of a dye suspension are prepared con.- taining 15 kilograms of a red-brown dye commercially available as Indanthren red-brown RR (see Schultz, Farbstoiftabellen, 7th edition, supplement Volume II, 1939, p. 204), Which dye is in a state of very fine dispersion. In addition, the suspension contains 1.32 kilograms monochloroacetic acid, 0.41 kilogram of the ammonium salt of dodecylbenzenesulfo acid, the rest being water, so as to obtain a total of 300 kilograms.

A stretch of 1,000 meters of a heavy popeline cloth of a type adapted for tailoring heavy top coats therefrom and having a weight of 350 grams per meter are processed in a fculard unit or a similar padding device known per se and are padded with the aforedescribed dye suspension at a temperature of 50. The squeeze effect is 70% and the cloth is passed through the padding unit at a rate of 50 meters per minute.

After this impregnation the cloth is passed to a cylinder dryer equipped with drums composed of precious steel or having another known acid-resistant coating. Upon this dryer the cloth is subjected to an intermediate drying process. The dye pigment is and remains entirely uniformly distributed throughout the fabric of the cloth and does not migrate to the surface portions of the fabric adjacent to the surface of the dryer drums.

The cloth is then conducted through a second impregnating unit at room temperature, which unit is supplied, step by step, with 300 liters of a liquor containing 18 liters of a solution of caustic soda having 38 B6. and 12 kilograms of sodiumhydrosulfite, the rest being water, so as to obtain a total of 300 liters. The cloth is thus treated with this liquor which reduces and fixes the pigment particles in the cloth.

Immediately thereafter the cloth is passed for a period of 30 seconds through a high-speed steaming unit where it is steamed at a temperature of from 102-109. The cloth is then rinsed, oxodized and soaped.

As a result, a cloth is obtained having a fabric being integrally dyed and wherein the dye pigments are very uniformly distributed throughout the entire fabric, thereby giving an appearance of a very uniform and even coloring on the upper as well as on the lower surface and also throughout the interior of the fabric.

Example II Example III Example I is repeated with the exception that the 0.41 kilogram of the ammonium salt of the dodecylbenzenesulfo acid in the dye suspension of Example I are replaced by an equal amount of the sodium salt of dioctylbenzenesulfo acid. The same advantageous dyeing effect is obtained as in Example I.

Example IV Example I is repeated with the exception that the 1.32 o

kilograms of monochloroacetic acid in the dye suspension of Example I are replaced by an equal amount of )8- chloropropionic acid. The same advantageous dyeing effect is obtained as in Example I.

Example V 300 kilograms of a dye suspension are prepared containing 9.00 kilograms of a blue dye commercially available as Indanthren blue BC (see Schultz, Farbstoiftabellen, seventh edition, supplement volume II, 1939, p. 198), the dye being in the state of a very fine dispersion. In addition, the suspension contains 1.30 kilograms of lactic acid as well as 0.40 kilogram of the sodium salt of oxystearic acid-N ethylanilide-sulfo acid ester, the rest being Water, so as to obtain a total of 300 kilograms.

A stretch of 1,000 meters of a staple fiber fabric having portions of varying density are processed in a foulard unit or a similar impregnating device and are padded with the aforementioned dye suspension at a temperature of 50. The squeeze effect is 70% and the fabric is passed through the impregnating unit at a rate of 50 meters per minute.

The cloth is then subjected to an intermediate drying process in a hotflue unit. There does not occur any migration of the dye pigment.

The cloth is then further processed as described in Example I after an intermediate drying.

As a result, a dyed fabric is obtained wherein the dye pigments are entirely evenly distributed and having an appearance of an entirely uniformly and evenly colored product.

Example VI Example V is repeated with the exception that instead of the sodium salt of the oxystearic acid-N ethylanilidesulfo acid ester the corresponding amount of a higher molecular alkyl sulfonate is used. The same advantageous coloring effect is obtained as in Example V.

Example VII Example V is repeated, however, without adding to the padding suspension the sodium salt specified therein. As a result, there occurs during the drying process a considerable migration of dye pigments from the denser portions of the fabric, drying comparatively slow, to the thin portions of the fabric which dry much faster. Consequently, the end product is very unevenly colored.

Example VIII 1.500 kilograms of a dye liquor are prepared, contaming 2.00 kilograms of a brown dye commercially available as Indanthren BR (see Schultz, Farbstofftabellen, seventh edition, supplement volume II, 1939, p. 203), which dye is also extremely finely dispersed. In addition, the liquor contains 2.50 kilograms of formic acid, 0.76 kilogram of the ammonium salt of dodecylbenzenesulfo acid and 30.00 kilograms of Glaubers salt (sodium sulfate decahydrate), the rest being water, so as to obtain a total of 1.500 kilograms.

kilograms of cotton are then treated on a dyeing unit known per se with the aforementioned dye liquor, the liquor ratio being 1:15. The dyeing is started at a temperature of 30 and the temperature is raised to 70 within a period of 20 minutes. At this temperature of 70 the dye liquor is retained in circulation for about 15 to 20 minutes, until the pigments of the liquor both have been fully extracted.

To this spent dye liquor there are then added 27 liters of a solution of caustic soda having 38 B. and 6 kilograms of sodium hydrosulfite with which the treatment of the fabric is continued for about 20 minutes, thereby reducing and fixing the pigment in the fibers. As a result of this process an entirely evenly and uniformly dyed product is obtained.

Example IX Example VIII is repeated, however, without adding the ammonium salt of the dodecylbenzenesulfo acid to the dye liquor. It is not possible to extract all pigments from the liquor and after adding the solution of caustic soda and the sodium hydrosulfite the pigment still retained in the liquor instantaneously enters the fibers without, however, distributing evenly therethrough. Consequently, a very uneven coloring effect is obtained.

It Will be understood that this invention is susceptible to further modification and, accordingly, it is desired to comprehend such modifications within this invention as may fall within the scope of the appended claims.

What is claimed is:

1. A dye liquor comprising a highly dispersed vat dye pigment, sufficient halogenated carboxylic acid to yield a pH between 2 and 4, and an anionic surface-active substance selected from the group consisting of alkyl sulfonic acids, sulfuric acid esters of oxystearic acid amides, sulfo succinic acid esters, alkyl benzene sulfonic acids and the corresponding salts thereof.

2. A dye liquor comprising a highly dispersed vat dye pigment, sufficient halogenated carboxylic acid to yield a between 2 and 4, and an alkyl benzene sulfonic aci 3. A dye liquor comprising a highly dispersed vat dye pigment, sutficient monoch oracetic acid to yield a pH between 2 and 4 and a dodecylbenzene sulfonic acid.

4. The dye liquor of claim 3 wherein there is sufiicient monochloracetic acid to yield a pH between 2.5 and 3.

5. A dye liquor comprising a highly dispersed vat dye pigment, a halogenated carboxylic acid in suiiicient amounts to yield a pH between 2 and 4; and a salt of an alkyl benzene sulfonic acid.

6. A dye liquor comprising a highly dispersed vat dye pigment, monochloro acetic acid, a halogenated carboxylic acid in sufficient amounts to yield a pH between 2 and 4; and a salt of dodecylbenzene sulfonic acid.

7. A method of dyeing cellulose textile materials, which method comprises the step of dyeing said cellulose matcrlals with a vat dye pigment liquor containing a highly dispersed vat dye pigment; sufiicient acid to equal a pH between 2 and 4, said acid being selected from the group consisting of formic acid, acetic acid, glycolic acid, lactic acid, halogenated carboxylic acids and aromatic sulfonic acids; and an anionic surface-active substance selected from the group consisting of alkyl sulfonic acids, sulfuric acid esters of oxystearic acid amides, sulfo succinic acid esters, alkyl benzene sulfonic acids and the corresponding salts thereof.

8. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a vat dye pigment liquor containing a highly dispersed vat dye pigment, a halogenated carboxylic acid in suflicient amounts to equal a pH between 2 and 4; and an anionic surface-active substance selected from the group consisting of alkyl sulfonic acids, sulfuric acid esters of oxysteearic acid amides, sulfo succinic acid esters, alkyl benzene sultonic acids and the corresponding salts thereof.

9. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a vat dye pigment liquor containing a highly dispersed vat dye pigment, a halogenated carboxylic acid in sufficient amounts to equal a pH between 2 and 4; and an alkyl benzene sulfonic acid.

10. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a vat dye pigment liquor containing a highly dispersed vat dye pigment, a halogenated carboxylic acid in sufilcient amounts to equal a pH between 2 and 4; and a salt of alkyl benzene sulfonic acid.

11. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a vat dye pigment liquor containing a highly dispersed vat dye pigment, monochloro acetic acid in sufficient amounts to equal a pH between 2 and 4; and an alkyl benzene sulfonic acid.

12. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a vat dye pigment liquor containing a highly dispersed vat dye pigment, monochloro acetic acid in sutlicient amounts to equal a pH between 2 and 4; and a salt of an alkyl benzene sulfonic acid.

13. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a vat dye pigment liquor containing a highly dispersed vat dye pigment, monochloroacetic acid in sufficient amounts to equal a pH between 2 and 4; and dodecylbenzene sulfonic acid.

14. A method of dyeing cellulose textile materials which method comprises the step of dyeing said cellulose material with a va-t dye pigment liquor containing a highly dispersed vat dye pigment, monochloroacetic acid in sufficient amounts to equal a pH between 2 and 4; and a salt of dodecylbenzene sulfonic acid.

References Cited in the file of this patent UNITED STATES PATENTS 2,346,473 Dahlen et al Apr. 11, 1944 2,518,393 Smith Aug. 8, 1950 2,982,597 Salvin et al. May 2, 1961 OTHER REFERENCES Goldsmith: Chem. Ind., March 1943, pages 326-328.

Color Index, A.A.T.C.C., Lowell, Mass, 1956, vol. 1 page 1673.

American Dyestuif Reporter, vol. 48, No. 7, April 1959, pages 41 and 43. 

1. A DYE LIQUOR COMPRISING A HIGHLY DISPERSED VAT DYE PIGMENT, SUFFICIENT HALOGENATED CARBOXYLIC ACID TO YIELD A PH BETWEEN 2 AND 4, AND AN ANIONIC SURFACE-ACTIVE SUBSTANCE SELECTED FROM THE GROUP CONSISTING OF ALKYL SULFONIC ACIDS, SULFURIC ACID ESTERS OF OXYSTEARIC ACID AMIDES, SULFO SUCCINIC ACID ESTERS, ALKYL BENZENE SULFONIC ACIDS AND THE CORRESPONDING SALTS THEREOF. 